CN114538414B - Synthesis method of single-walled carbon nanotube fiber - Google Patents
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Abstract
The invention discloses a synthesis method of single-walled carbon nanotube fibers, and belongs to the technical field of chemistry. The method of the invention uses radio frequency plasma to decompose ferric chloride (catalyst), thiophene (catalyst auxiliary agent) and coal tar (carbon source), and carries out vapor deposition in a vertical furnace to synthesize the single-walled carbon nanotube fiber. The method has simple flow, higher production efficiency compared with the existing floating catalysis method, and cheap raw materials, is suitable for fibrous single-walled carbon nanotubes with lower production cost, and is used for manufacturing special cables and conductive agents for lithium batteries.
Description
Technical Field
The invention relates to a synthesis method of single-walled carbon nanotube fibers, and belongs to the technical field of chemistry.
Background
The carbon nanofibers and carbon nanotubes have similar microstructure morphology and properties, which determine their excellent physical and chemical properties. Therefore, the carbon nanofiber has wide application potential in the aspects of lithium ion battery materials, super capacitor materials, sensing materials, intelligent materials, devices thereof and the like. In recent years, carbon nanotubes have been widely used in the new energy automobile lithium ion battery industry as an excellent conductive agent. The capacity, the service life and the safety of the lithium battery are obviously improved. With the requirements of high energy density, safer and higher-rate charge and discharge and the like of a lithium ion battery by a new energy automobile, the performance improvement of the lithium ion battery is urgent. Compared with multi-wall carbon nanotubes, the single-wall carbon nanotubes have higher length-diameter ratio, better mechanical strength and higher flexibility. The conductive agent is added into the anode and cathode materials, so that a stable and rich conductive network can be provided in the lithium intercalation and deintercalation process, and the mechanical property of the pole piece is effectively improved. Because the single-wall carbon nanotube fiber and the single-wall carbon nanotube have similar structures and properties, the single-wall carbon nanotube fiber and the single-wall carbon nanotube can be used as high-efficiency conductive agents to be applied to anode and cathode materials of lithium ion batteries.
The research and development of the carbon nanofibers and the carbon nanotubes are synchronous, the preparation methods are basically the same, and specific preparation processes are different. At present, the synthesis method of single-wall carbon nanotubes is mainly an arc discharge method, and graphite with a distance of a few millimeters generates arc discharge under the action of strong current in an inert atmosphere, consumes an anode and forms carbon deposits on the surface of a cathode. The method has high energy consumption and low yield, so that a synthetic method with lower development cost is very important for the application of single-wall carbon nanotubes in a wider range.
Compared with the arc discharge method, the CVD method has become the mainstream method for the laboratory and industrial production of the carbon nano tube because of the advantages of simple equipment, lower temperature, easy parameter control and the like. In the CVD method, a plasma source is introduced, and electrons with high energy are contained in the plasma and collide with molecules in gas phase to provide activation energy required by a vapor phase CVD reaction, so that the decomposition and ionization processes of gas molecules are promoted, and high-activity chemical groups are generated. Further reduces the temperature of the CVD reaction and improves the reactivity.
Disclosure of Invention
The invention provides a synthesis method of single-walled carbon nanotube fibers, which comprises the following steps:
(1) Dispersing ferric salt and thiophene in ethanol to prepare a catalyst system, and placing the catalyst system in a raw material storage tank 1; coal tar is taken as a carbon source and added into a raw material storage tank 2;
(2) Helium is introduced into a hearth of the CVD device, and the temperature is controlled to be 1000-1300 ℃; simultaneously pumping the catalyst system in the raw material storage tank 1 and the carbon source of the raw material storage tank 2 into an ultrasonic atomizer, and respectively introducing the atomized catalyst system and carbon source into a hearth of the CVD device by taking hydrogen and helium as carriers;
(3) A plasma torch is arranged in a hearth of the CVD device, and after an atomized catalyst system and a carbon source enter the plasma torch, a radio frequency power supply starts to work to drive the plasma torch to decompose raw materials, and single-wall carbon nano tube fibers are obtained through vapor deposition growth in the furnace.
In one embodiment of the invention, the concentration of iron salt in the catalyst system is from 0.5 to 0.6g/mL; the concentration of thiophene is 0.16-0.25g/mL.
In one embodiment of the invention, the mass ratio of iron salt to thiophene is (2-4): 1.
in one embodiment of the invention, the iron salt may be selected from ferric chloride.
In one embodiment of the invention, the flow rate of the atomized catalyst into the furnace chamber of the CVD device is 8-10mL/min; the flow rate of the atomized carbon source introduced into the hearth of the CVD device was 300mL/min.
In one embodiment of the present invention, 3000sccm hydrogen and 1000sccm helium are used as carriers in step (2).
In one embodiment of the invention, the rf power driving conditions of the plasma torch in step (3) are: the power is 5-8kW, and the frequency is 10-15MHz.
In one embodiment of the invention, the specific steps of the method shown are as follows:
1) Weighing ferric chloride and thiophene, adding the ferric chloride and the thiophene into an ethanol solution, stirring and dissolving the ferric chloride and the thiophene, and adding the ferric chloride and the thiophene into a raw material storage tank 1 of CVD equipment; weighing coal tar as a carbon source, and adding the coal tar into a raw material storage tank 2;
2) Heating to 1200 ℃ in a CVD furnace under the condition of introducing helium; then the raw materials in the storage tank 1 and the storage tank 2 are pumped into an ultrasonic atomizer at the same time; after the raw materials are pumped into an ultrasonic atomizer, the ultrasonic atomizer starts to work, and 3000sccm hydrogen and 1000sccm helium are taken as carriers, so that atomized raw materials are brought into a plasma torch;
3) After the atomized raw materials enter the plasma torch, the radio frequency power supply starts to work, the plasma torch is driven to decompose the raw materials, and single-wall carbon nano tube fibers are grown in the furnace through vapor deposition; and cooling the grown single-walled carbon nanotube fiber through a stainless steel water cooling jacket at the lower end, and collecting the product.
The invention also provides a single-walled carbon nanotube fiber based on the preparation method.
The invention also provides application of the single-walled carbon nanotube fiber in lithium ion battery materials, super capacitor materials, sensing materials and intelligent materials.
Advantageous effects
The invention uses radio frequency plasma to decompose ferric chloride (catalyst), thiophene (catalyst auxiliary agent) and coal tar (carbon source), and synthesizes single-wall carbon nano tube fiber by vapor deposition in a vertical furnace. The method has simple flow, higher production efficiency compared with the existing floating catalysis method, and cheap raw materials, is suitable for fibrous single-walled carbon nanotubes with lower production cost, and is used for manufacturing special cables and conductive agents for lithium batteries.
Drawings
FIG. 1 is a scanning electron microscope image of the single-walled carbon nanotube fiber obtained in example 1, magnified 100000 times.
FIG. 2 is a scanning electron microscope image of the single-walled carbon nanotube fiber obtained in example 1 at 1000000 Xmagnification.
Detailed Description
The coal tar related in the embodiment of the invention is purchased from Hubei Weikun energy low-temperature coal tar B0029.
Example 1
26.3g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to 8mL/min, the flow rate of the atomized coal tar was controlled to 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Example 2
26.3g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 9mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, the mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei bright power low-temperature coal tar b0029. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Example 3
30g of ferric chloride and 8g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to 9mL/min, the flow rate of the atomized coal tar was controlled to 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The coal tar is purchased from Hubei Weikun energy sources, low-temperature coal tar b0029, a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz is used for driving a plasma torch, reaction raw materials are fully atomized by ultrasonic waves and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Example 4
30g of ferric chloride and 8g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 10mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, the mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei bright power low-temperature coal tar b0029. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Example 5
25.2g of ferric chloride and 8.4g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution is controlled to be 10mL/min, the flow rate of the atomized coal tar is controlled to be 300mL/min, the mixed gas of 3000sccm hydrogen and 1000sccm helium is used as carrier gas, and the coal tar is purchased from Hubei bright power low-temperature coal tar b0029. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Comparative example 1:
with reference to example 1, only the catalyst solution flow rate was changed from 8mL/min to 20mL/min, as follows:
26.3g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to be 20mL/min, the flow rate of the atomized coal tar was controlled to be 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The coal tar is purchased from Hubei Weikun energy source low-temperature coal tar b0029. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Comparative example 2:
with reference to example 1, the mass of the weighed ferric chloride was merely changed to 6g, and the concrete steps were as follows:
6g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of coal tar was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to 8mL/min, the flow rate of the atomized coal tar was controlled to 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The coal tar is purchased from Hubei Weikun energy source low-temperature coal tar b0029. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Comparative example 3:
referring to example 1, benzene was selected as the carbon source for the reaction.
26.3g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of benzene was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to 8mL/min and the flow rate of the atomized benzene was controlled to 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Comparative example 4:
referring to example 1, cyclohexane was selected as a carbon source during the reaction, and the following is concrete:
26.3g of ferric chloride and 12.5g of thiophene are weighed, 50g of ethanol is added, and the mixture is stirred and dissolved to be used as a catalyst solution. 3kg of cyclohexane was weighed as a carbon source.
A corundum tube vertical furnace with the pipe diameter of 100mm and the height of 1500mm is used as a reactor, and the furnace is heated to 1200 ℃ under the blowing of helium and then is insulated. The catalyst solution and the carbon source were placed in the storage tank 1 and the storage tank 2, respectively, and pumped into an ultrasonic atomizer, respectively, and the atomized raw material was brought into a plasma torch by using a mixed gas of 3000sccm hydrogen and 1000sccm helium as a carrier gas. The flow rate of the atomized catalyst solution was controlled to 8mL/min and the flow rate of the atomized cyclohexane was controlled to 300mL/min, and a mixed gas of 3000sccm hydrogen and 1000sccm helium was used as a carrier gas. The plasma torch is driven by a radio frequency power supply with the power of 5kW and the frequency of 13.56MHz, the reaction raw materials are fully atomized by ultrasonic and then enter the plasma torch to be decomposed, single-wall carbon nano tube fibers are synthesized by vapor deposition in a vertical furnace, and reaction products are collected after being cooled by a stainless steel water cooling jacket at the lower end.
Performance test:
after the reaction, the collected carbon nanotube fibers were weighed. The carbon nanotube powder was obtained by mechanical pulverization, and a slurry (97.5% NMP+2% CNT+0.25% dispersant+0.5% PVP) was prepared. The resistivity after coating was tested, the ratio of 7.5g slurry +50g HSV +15.6g LCO, and the addition of CNT was 0.3%. The test results are shown in table 1:
TABLE 1 Properties of carbon nanotube fibers obtained by different methods
| Carbon nanotube fiber | Mass/g | Resistivity/Ω·cm |
| Example 1 | 215.21 | 8.06 |
| Example 2 | 217.32 | 9.23 |
| Example 3 | 216.5 | 8.29 |
| Example 4 | 217.27 | 8.47 |
| Example 5 | 216.89 | 8.5 |
| Comparative example 1 | 164.2 | 16.25 |
| Comparative example 2 | 179.83 | 15.21 |
| Comparative example 3 | 168.67 | 16.36 |
| Comparative example 4 | 189.35 | 25.37 |
As can be seen from the table, comparative example 1 changed only the flow ratio of catalyst to carbon source, comparative example 2 changed only the ratio of ferric chloride to thiophene, and the yield of carbon tube was lowered and the conductivity was deteriorated after the change, compared with example 1. Comparative example 3 changed only carbon source to benzene, comparative example 4 changed only carbon source to cyclohexane, and the yield of carbon tubes was lowered and the conductivity was deteriorated as compared with example 1.
Claims (6)
1. The synthesis method of the single-walled carbon nanotube fiber is characterized by comprising the following steps:
(1) Dispersing ferric salt and thiophene in ethanol to prepare a catalyst system, and placing the catalyst system in a first raw material storage tank (1); adding coal tar serving as a carbon source into a second raw material storage tank (2);
(2) Helium is introduced into a hearth of the CVD device, and the temperature is controlled to be 1000-1300 ℃; simultaneously pumping a catalyst system in a first raw material storage tank (1) and a carbon source of a second raw material storage tank (2) into an ultrasonic atomizer, and respectively introducing the atomized catalyst system and carbon source into a hearth of a CVD device by taking hydrogen and helium as carriers;
(3) A plasma torch is arranged in a hearth of the CVD device, and after an atomized catalyst system and a carbon source enter the plasma torch, a radio frequency power supply starts to work to drive the plasma torch to decompose raw materials, and single-wall carbon nano tube fibers are obtained through vapor deposition growth in the furnace;
wherein, in the step (1), the mass ratio of the ferric salt to the thiophene is (2-4): 1, a step of; the radio frequency power driving condition of the plasma torch in the step (3) is as follows: the power is 5-8kW, and the frequency is 10-15MHz.
2. The process according to claim 1, wherein the concentration of iron salt in the catalyst system is 0.5-0.6g/mL; the concentration of thiophene is 0.16-0.25g/mL.
3. The method according to claim 1, wherein in the step (2), the flow rate of the atomized catalyst into the furnace chamber of the CVD apparatus is 8-10mL/min.
4. The method according to claim 1, wherein in the step (2), the flow rate of the atomized carbon source into the furnace chamber of the CVD apparatus is 300mL/min.
5. The method of claim 1, wherein 3000sccm hydrogen and 1000sccm helium are used as carriers in step (2).
6. The method of any one of claims 1-5, wherein the iron salt is ferric chloride.
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| CN101195482B (en) * | 2007-12-10 | 2011-01-26 | 北京大学 | Method for growing semiconductor single-wall carbon nano-tube |
| CN101209835A (en) * | 2007-12-21 | 2008-07-02 | 北京大学 | Method for synthesizing thin wall carbon nano-tube |
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| CN104555989B (en) * | 2015-01-30 | 2016-06-15 | 西安科技大学 | A kind of method adopting coal tar to prepare CNT |
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| KR20220032118A (en) * | 2017-08-22 | 2022-03-15 | 테르마 코퍼레이션 | Graphene nanoribbons, graphene nanoplatelets and mixtures thereof and methods of synthesis |
| CN110155986B (en) * | 2018-02-13 | 2023-01-13 | 中国科学院金属研究所 | Preparation of single-walled carbon nanotube transparent conductive film with single or small tube bundle size |
| CN111348642B (en) * | 2020-04-23 | 2022-03-08 | 无锡东恒新能源科技有限公司 | Device and method for preparing single-walled carbon nanotube by floating catalysis method |
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